Process of making aluminum chloride



' yJulyll, 1931. A. McD. McAFEE 'PROCESS OF-MAKING ALUMINUM CHLORIDE Filed June` 1,-1927 Patented y July 14, 1931 UNITED vSTATES PATENT or'rlca ALMER MCDUFFIE MCAAFEE, OF PORT ARTHUR, TEXAS,v ASSIGNOR TO GULF .REFINING COMPANY, PITTSBURGH, PENNSYLVANIA, A CORPORATION OF TEXAS PROCESS 0F MAKING ALUMINUM CHLORIDE i Appiication mea June 1, 1927. serial No. 195,77a`

This invention relates to processes of making aluminum chloride; and it comprises .a method of making aluminum chloride from carbon and raw bauxitewherein calcined bauxite and carbon are mixed, the mixture carbonized and introduc'edwhile hot into a previously heated .columnar chamber at ya temperature suiiicifent to induce and continue the aluminum chloride forming reaction, the

introduced material formin'a pervious column, usually vertical, of su stantial length and a current of chlorin is fed through the K column at the maximum speed consistent with substantially complete absorption, passage of chlorin in this manner being continued until substantial quantities of chlorin appear in the` effluent gases and vapors, at which time the ow of chlorin is interrupted,

the length ofthe column restored by adding further quantities of carbon and bauxite,'and the flow of chlorin resumed; all as more fully hereinafter set forth and as claimed.

The formation of vapors of aluminum chloride by treating a hot mixture of alumina and carbon with chlorin is a very old reaction; one which has been-utilized for many years, although the exact chemistr reactions involved is not, even yet, efinitely settled. Although the reaction requires a relatively high temperature (say 10001200 F.) to inaugurateand continue it, no great quantity of heat is needed; that is, after the materials are at reacting temperature, no

great amountof heat is absorbed'.` Really, I find, with bauxite and carbon.

the reaction, and chlorin is exothermic as a whole; that is, y some heat is liberated in spite of the fact that two solid bodies, namely, vcarbon and alumina, are converted into gas and vapor. The amount of heat evolved depends upon the relative proportions of carbon and alumina and is greatest when the carbon islimited so as to allow' CO2 gases. On the other hand, to insure complete reaction, an ample supplyv of carbon is advisable. Under all circumstances however,

the fact is as stated: with thematerials at' reaction temperature andwith loss of heat by radiation restricted, the reaction 1n general willkeep itself going. In theprior "speak,

to appear in the elux to utilize the exothermic nature of the reaction to make it self-supporting, that is to obviate the use of heat from an external source. This renders the whole operation and the apparatus used simpler and more practicable. One of these expedients is a rapid rate of reaction; supplying a rapid wflow of chlorin to the apparatus; and, so to driving the action. The radiation loss in a time unit per square foot of exposed surface at a given temperature is constant, irrespective of the amount of reaction going 0n within theapparatus. If the rate of this reaction is suiiiciently rapid, as compared with the area of`heat radiating surface,1the l.

development of heat incident tothe reaction forming aluminum chloride suiices to compensate for losses and the sensible heat carvried away in effluent gases and vapors, and

the reaction then goes ahead without any necessity forthe supply of heat from external sources. A heightened ratio of heat development to radiating area can be secured by 1n- 'creasing the diameter of the apparatus, as

' well as by mcreasing the rapidity of the iow of chlorin and by suiiiciently protecting all exposed surfaces against the loss of heat. In l I use all three expedients.

Furthermore, I customarily Vemploy calcined bauxite in lieu of pure alumina. With bauxite calcined around 1800 F., the reaction, ent (iron, more exothermic than with pure alumina. Calcination is necessary to remove moisture, which isextremely detrimental in this reaction.

I consider my invention as covering a pract1ce,

l process of producing aluminum chloride Yabecause of various impurities pres silica, T102 etc.), 1s somewhat `to have some proportion of coa-rse or lum pors from bauxite, carbon and. chlorin which is thermally self-supporting; in which the.

- The shaft is now refilled with a hot charge reaction mass keeps alive and the reaction goes forward without heat to the reaction chamber.

In a practical embodiment ofthe present invention, I calcine raw bauxite, which may be run-of-mine material, in any suitable way and finely grind it, mixing it with finely ground coking coal. Fine grinding may precede calcination. From thismixture I make briquets, ordinarily employing a small amount of wax tailings or other suitable binder. The briquets are shaped, ressed and baked in an ordinary way; the ba ing or carbonization being at a rather high tempera-y ture to get rid, so far as possible, of all hydrocarbons and volatile matters. A temperature of 12000-1500o ized material is supplied directly to the reartion chamber, its sensible heat is utilized.

While I find it advantageous to mix, briquet and carbonize as described, calcination of the bauxite and carbonization of the coal to give coke may be separately performed and the two hot materials introduced into the reaction chamber without any very intimate mixing. It is, in fact, found better bauxite to maintain permeability of the charge, if'the rest of the vcharge is fine. One ofthe reasons for using briquets is to secure permeability of the column. y

For the manufacture of aluminum chlorlde, I lcustomarily employ a vertical shaft chamber of brickwork or the like as a. reaction chamber, this shaft being heat insulated as far as possible. I do not desire to make it less than about 3 feet in diameter; and greater diameters are better. Assuming that. such an apparatus is to be put in operation, I first heat it up in an ordinary way. For example, a fire of wood, followed b coke,`may be built in the shaft, the top and bottom being) open for draft. A flame of oil or gas may e usedfor heating. After the shaft walls are sufficiently heated, the interior temperature being at least 1000 F., I introduce a charge of material into the shaft on top of such coke as may then remain from the preliminary heating up operation. This coke, at this time, is emitting carbon monoxid and carbon dioxid, which permeate'the body of introduced material and assist in initiatmg reaction. Through the column of hot material, I pass chlorin as rapidly as is compaisible with a substantially complete utilizatlon; i. e., so thatthe tail gases going beyond the condenser do not show, say, more than 1 per cent of free chlorin.

c hlorin is continued at this chlorin in proportions above the limit set begins to appear in the tail gases. I ordinar1l pass the'chlorin downward through the umn. At the time when chlorin beyond Introduction of a supply of external F. will serve. If the carbonrapid rate until the limit begins to appear, the column has wasted away and is now relatively short.

vapors produced in treating crude bauxite usually contain silicon chloride and titanium chloride which go through the condenser unchanged, I usually lead the eiiluent gases and vapors from the aluminum chloride condenser finally through some type of scrubber to get rid of these bodies.

In the accompanying illustration, I have shown, more or less diagrammatically, c ertain apparatus capable of use in performing the present invention. In this showing,

The figure is a view in central vertical section of a complete apparatus, certain parts being shown in elevation.

As shown, l is a tower of ordinary masonry. Fire brick serve well. This is surrounded by layer 2 of suitable heat insulating material, such as kieselguhr, powdered bauxite, etc., and an external jacket 3 of iron or steel. At the top, it is closed by cover 4 which can be readily removed for inspection P or repairs. Element 5 is a retort head allowing introduction of solid materials and elevment 6 is a valved pipe for introduction of y stirring mechanism and both opening at their bases into collection chamber 15. Aluminum chloride vapors vpass downward through the irst chamber 1'3 and upward through the second chamber 14. Eluent gases and vapors pass through conduit 16 into the base of a diagrammatically shown scrubber 17 having water introducing means 18 near its top.

In the use of this apparatus, tower 1 having been heated in a manner previously described, to a temperature of 1000 F. or thereabouts, is filled with a charge of reaction material produced as previously described, up to a point just below the top and downward introduction of chlorin begun. Aluminum chloride vapors are formed and pass forward through the condensing apparatus. waste gases passing to the scrubbing tower are tested from time to time. Flow of chlorin is continued until a trace of chlorin shows up in the waste'gases. The iiow of chlorin is then interrupted.- The tower is again filled The with fresh, hot aluminous material opto and through the charge at as rapid a rate as is consistent with substantially complete Y utilization of such chlorin, interrupting the feed of chlorin when free chlorin in amount over about one per cent appears in the eiuent vapors, restoring the initial height of the co1- umn by charging fresh hot bauxite and carbloi thereto and resumm' g the rapid feed of c orm.

In testimony whereof, Iihave'hereunto af fixed my si ature.

R MCDUFFIE MOAFEE. 

